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Practical Chemistry
Practical Chemistry
Practical Chemistry
Introduction
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A burette is used to deliver solution in precisely measured, variable volumes. Burettes are
used primarily for titration, to deliver one reactant until the precise end point of the
reaction is reached. To fill a burette, close the stopcock at the bottom and use a funnel. You
may need to lift up on the funnel slightly, to allow the solution to flow in freely.
You can also fill a burette using a disposable transfer pipette. This works better than a
funnel for the small, 10 mL burettes. Be sure the transfer pipette is dry or conditioned with
the titrant, so the concentration of solution will not be changed.
Before titrating, condition the burette with titrant solution and check that the burette is
flowing freely. To condition a piece of glassware, rinse it so that all surfaces are coated
with solution, then drain. Conditioning two or three times will insure that a stray drop of
water does not change the concentration of titrant.
Rinse the tip of the burette with water from a wash bottle and dry it carefully. After a
minute, check for solution on the tip to see if your burette is leaking. The tip should be
clean and dry before you take an initial volume reading.
When your burette is conditioned and filled, with no air bubbles or leaks, take an initial
volume reading. A burette-reading card with a black rectangle can help you to take a more
accurate reading. Read the bottom of the meniscus. Be sure your eye is at the level of
meniscus, not above or below. Reading from an angle, rather than straight on, results in a
parallax error.
Deliver solution to the titration flask by turning the stopcock. The solution should be
delivered quickly until a couple of mL from the endpoint. The endpoint should be approached
slowly, a drop at a time. Use a wash bottle to rinse the tip of the burette and the sides of
the flask. Your TA can show you how to deliver a partial drop of solution, when near the
endpoint.
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Erlenmeyer flasks and beakers are used for mixing, transporting, and reacting, but not for
accurate measurements. The volumes stamped on the sides are approximate and accurate to
within about 5%.
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Start by squeezing the bulb in your preferred hand. Then place the bulb on the flat end of
the pipette.
Place the tip of the pipette in the solution and release your grip on the bulb to pull solution
into the pipette. Draw solution in above the mark on the neck of the pipette. If the volume
of the pipette is larger than the volume of the pipette bulb, you may need to remove the
bulb from the pipette and squeeze it and replace it on the pipette a second time, to fill the
pipette volume completely.
Quickly, remove the pipette bulb and put your index finger on the end of the pipette. Gently
release the seal made by your finger until the level of the solution meniscus exactly lines up
with the mark on the pipette. Practice this with water until you are able to use the pipette
and bulb consistently and accurately.
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To make up a solution, first dissolve the solid material completely, in less water than
required to fill the flask to the mark.
After the solid is completely dissolved, very carefully fill the flask to the 500 ml mark.
Move your eye to the level of the mark on the neck of the flask and line it up so that the
circle around the neck looks like a line, not an ellipse. Then add distilled water a drop at a
time until the bottom of the meniscus lines up exactly with the mark on the neck of the
flask. Take care that no drops of liquid are in the neck of the flask above the mark.
After the final dilution, remember to mix your solution thoroughly, by inverting the flask
and shaking.
Do check the level indicator bubble before weighing. The two rear balance feet serve as
levelling screws. Use the brush provided to clean spills in the weighing chamber. Discard any
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disposable tare containers or weighing paper, in the nearest wastebasket.
(g) Calorimetry
Calorimetry is used to determine the heat released or absorbed in a chemical reaction. The
calorimeters shown here can determine the heat of a solution reaction at constant
(atmospheric) pressure. The calorimeter is a double Styrofoam cup fitted with a plastic top
in which there is a hole for a thermometer.
(It's crude, but very effective!) Key techniques for obtaining accurate results are starting
with a dry calorimeter, measuring solution volumes precisely, and determining change in
temperature accurately.
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button to zero the balance. Carefully add substance to the container or paper. Record the
mass. Use the brush provided to clean any spills. Discard any disposable tare containers or
weighing paper in the nearest wastebasket.
Quantitative Transfer
Quantitative Transfer simply means that all the material to be transferred from one place
to another must make the trip. For example, every particle of solid must be transferred
from the weighing paper to the (clean) beaker.
This can be done be carefully tipping the creased weighing paper to pour the solid into the
beaker. Tapping the paper with a spatula will knock particles into the beaker.
Finally, the paper should be rinsed into the beaker, to remove all traces of the solid.
Titration
A titration is a method of analysis that will allow you to determine the precise endpoint of a
reaction and therefore the precise quantity of reactant in the titration flask. A burette is
used to deliver the second reactant to the flask and an indicator or pH Meter is used to
detect the endpoint of the reaction.
1. BUNSEN BURNER
(i) Close the air hole and turn the gas tap full on. Light the gas and hold a piece of wire in
different parts of the flame, moving it from the bottom to the top. Note the hottest place
in the flame. Open the air hole. Again hold the wire in the flame, moving from the bottom to
the top. Note the hottest place in the flame. Compare the two flames and note which has
the hottest point.
(ii) Close the air hole. Hold a test-tube with its bottom end just above the flame. Carbon
deposits on the glass. To test whether unburned carbon gives the yellow colour to the flame,
sprinkle powdered charcoal into the flame to see if this gives the same effect.
(iii) Open the air hole again. Note whether carbon deposits on a test-tube held in this flame.
Air mixing with the gas helps it to burn more rapidly and efficiently. To test what is in the
cooler inner cone hold a splint of wood in the flame so that it passes through the inner cone.
Note which part of the splint burns. Hold a piece of glass tubing with one end in the inner
cone then ignite the gas that comes out of the other end.
(iv) Investigate a candle flame and the flame of a spirit lamp in a similar way. Find the
hottest part of the flame. Test for unburned carbon particles in the flame. Look for an
inner cone of unburned gases.
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IDENTIFICATION OF PURE SUBSTANCES
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but does not touch, the bottom of the test-tube or flask. Add boiling chips to prevent
bumping. Boil the water and read the temperature on the thermometer. Stop heating.
Connect a water pump to the sidearm or to the second hole of the 2-hole stopper. When the
water stops boiling, turn on the water pump to reduce the pressure. Read the temperature,
heat to boiling and read the temperature again.
Temperature/OC 0 10 20 30 40 50 60
Solubility(g/100g 6.9 8.2 9.6 11.1 12.7 14.5 16.4
of water)
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iodide in 5 mL water. To each test-tube add iodine crystals, attach a stopper and shake.
Sodium chloride dissolves readily in water but not so readily in alcohol
DETERMINATION OF DENSITY
9(a) Density of a solid
The density of a solid is the ratio of mass to volume. We can find the density of a regular
solid with a balance and ruler. We can find the volume of an insoluble irregular solid with a
measuring cylinder. Half fill a graduated cylinder with water. Read the volume, immerse the
solid in the water and read the volume again. The difference in the two readings is the
volume of the solid.
SEPARATION OF MIXTURES
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(e) Separate two immiscible liquids of different density
Use a separating funnel or make a separating funnel with a piece of wide tubing fitted with
a stopper, tube and rubber tube with a clip. Shake the mixture thoroughly in a closed
container then run it into the separating funnel. Wait until a clear boundary appears
between the two liquids and then run off the denser layer into a beaker below.
Clean 25 cm of magnesium ribbon and cut into 1 cm pieces. Weigh a crucible plus lid, put the
pieces of magnesium ribbon in the crucible and weigh again. Put the crucible on a pipe clay
triangle supported on a tripod. Heat very gently then strongly. Hold the crucible lid in a pair
of tongs close to the crucible. The magnesium ribbon darkens just before it begins to melt.
At the first sign of burning, place the lid on the crucible and remove the Bunsen burner.
Every 4 seconds, raise the lid to allow more air to enter but do not allow any white
magnesium oxide smoke to escape. When the magnesium stops burning on raising the lid,
remove the lid. Heat the crucible again strongly but still hold the crucible lid in a pair of
tongs close to the crucible in case the magnesium starts to burn again. Leave the crucible to
cool. When cool, weigh the crucible plus lid plus contents. Calculate the increase in mass of
the magnesium.
(b) Substances that neither gain nor lose mass when heated
Weigh a test-tube containing 1 cm dry zinc oxide and a 1 cm plug of cotton wool at the
mouth to prevent loss of any solid during heating. Heat the test-tube and cotton wool and
weigh it again. Note any change in the zinc oxide. Note any loss in mass.
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Blue copper sulphate crystals + heat -> white, anhydrous copper sulphate + water.
This is a reversible change.
(b) Oxygen
(i) Prepare oxygen safely by decomposition of hydrogen peroxide solution. Put 20 mL
hydrogen peroxide into a 100 mL bottle. Fix a delivery tube to the bottle. Add two spatulas
of manganese dioxide and oxygen bubbles off for collection.
(ii) Oxygen is colourless and has no smell. To test whether the test-tube contains oxygen,
light a splint of dry wood, blow out the flame leaving a glowing splint then put the glowing
splint in a test-tube of oxygen. The glowing splint bursts into flame. This experiment is
called the glowing splint test.
(iii) Use an L-shape piece of nichrome wire with a shield to fit on the top to protect your
hand. Fix steel wool into a loop in the lower end of the Nichrome wire. Heat the steel wool
to red hot in a Bunsen burner flame then inserts it quickly into a test-tube of oxygen.
(iv) Fix a small piece of charcoal into the loop in the lower end of the Nichrome wire. Ignite
the charcoal in the Bunsen burner flame and then insert it quickly into another test-tube of
oxygen.
(v) Dip the loop in the lower end of the Nichrome wire into sulphur powder. Ignite the
sulphur powder in a Bunsen burner flame and then insert it quickly into another test-tube of
oxygen.
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(c) Hydrogen chloride
Put rock salt, sodium chloride, into a 100 mL filtering flask. Coarse rock salt causes less
frothing than the fine salt. Carefully add concentrated sulphuric acid down the thistle
funnel. You can collect hydrogen chloride gas by upward displacement of air, as in the
diagram.
(i) Collect four test tubes of the gas and cork them. Remove the cork from one of these
test tubes under water. Note the solubility of hydrogen chloride.
(ii) Hold a piece of cotton wool soaked in ammonium hydroxide at the mouth of a test-tube
of hydrogen chloride.
(iii) Shake a test-tube of the gas with water to obtain a solution of hydrogen chloride. Test
the solution with an acid/base indicator. Put a piece of magnesium ribbon in the solution.
Collect any gas formed and test for hydrogen with the glowing splint test.
(d) Ammonia
(i) Put a mixture of calcium hydroxide and ammonium chloride into a test-tube to a depth of
4 cm. Fill a U-tube with lumps of calcium oxide mixed with cotton wool. The cotton wool is to
prevent blocking of the tube. Gently heat the test-tube. The calcium oxide dries the
ammonia gas. Test whether the receiver test-tube is full by holding a piece of red litmus
paper at the opening. Collect test tubes of ammonia and cork them. The method of
collection illustrates that ammonia gas is lighter than air.
(ii) Fill a flask with ammonia. Fit a cork and tube into the flask as shown. The tube should
have been drawn out into a jet. Warm the flask gently to expand the gas and then hold the
flask upside down with the tube in the water. Water will spray into the flask from the jet.
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(ii) Make a sugar solution and half fill a jar with this solution. Add a spoonful of yeast and
leave to stand for 2 days. Construct a bubbler to fit on the top of the jar. Note whether
the yeast forms a gas. Note whether carbon dioxide gas collects in the upper part of the
jar.
12(a) RUSTING
Take 7 test tubes and 11 clean nails. Prepare the tubes as shown below:
Tube 1: Put 2 clean nails in the test-tube and half cover them with distilled water. These
nails are in contact with air and water and form the control experiment.
Tube 2: Put a few pieces of anhydrous calcium chloride or silica gel in the bottom of a dry
test-tube, and also two nails. Put a plug of cotton wool in the top of the tube. These nails
are in contact with air, but not moisture.
Tube 3: Boil water for several minutes to expel dissolved air and pour into the test-tube
whilst hot. Put 2 nails in the water. Put a little Vaseline or a few drops of olive oil on the
surface of the hot water. The Vaseline will melt and form an airtight layer, solidifying as
the water-cools. These nails are in contact with water but not air.
Tube 4: Half cover 2 nails with water containing a little common salt dissolved in it. These
nails are in contact with air, water and salt.
Tube 5: Wrap a piece of zinc foil round part of a nail. Put the nail in the test-tube and
almost cover with tap water.
Tube 6: Wrap a piece of tin foil round part of the nail. Put the nail in the test-tube and add
tap water as you did for tube 5.
Tube 7: Wrap a piece of copper wire round a nail and put it in the test-tube exactly like
tubes 5 and 6. Stand these 7 test tubes in a rack and leave for several days. Note the
conditions for rusting and which metal, (zinc, copper or tin), is best at preventing rusting.
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(a) Extract coloured substances from plants
Select brightly coloured flowers, such as the purple and red bougainvillaea, or coloured
leaves. Squeeze or grind one of the coloured flowers or leaves in a mortar with a mixture
made of 2 mL acetone and 2 mL ethanol. By this means the colouring matter will be
extracted into the solvent. Filter and collect the filtrate. Repeat this experiment with one
or two other flower colours. Keep these coloured solutions for use as "indicators" in the
next experiment.
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lemon juice, vinegar, sodium bicarbonate solution, washing soda, lime water, sodium
hydroxide solution, tap water, distilled water.
14. CRYSTALS
(a) Crystal growth
Sodium thiosulphate crystals grow rapidly from a super-saturated aqueous solution. The
formula for the crystals is Na2S2O3.10H2O. On heating, these crystals dissolve in some of
their water of crystallization. Put 3 cm of sodium thiosulphate crystals in a test-tube. Add
2 drops of water. Heat gently until all the crystals have dissolved. They appear to "melt".
Leave to cool. Crystals may not form unless you drop a tiny seed crystal of sodium
thiosulphate into the solution. Then crystal growth commences and spreads rapidly through
the whole solution. Watch the growth from one centre. Hold the tube in the hand while
crystallization occurs.
15. DIFFUSION
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(a) Diffusion of heavy carbon dioxide gas upwards
(i) Fill a jar with carbon dioxide and invert it over a similar jar full of air. After a few
moments separate the jars, pour a little lime water in the lower one and shake it. The lime
water will turn milky indicating that the carbon dioxide has fallen into the lower jar because
it is the heavier gas.
(ii) Repeat the experiment with the carbon dioxide in the lower jar and invert a jar of air on
top of it. If the jars are left for about 5 minutes carbon dioxide will be carried into the
upper jar by diffusion; in the same way air will be carried into the lower jar. The lime water
test will show the presence of carbon dioxide in the upper jar.
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and then touch the prepared water surface. The oil spreads out. Measure the approximate
area over which it spreads. Estimate what fraction of oil was removed by the glass point by
using the glass point to remove successive fractions from the drop until it has been used up.
The volume of oil put on the water can be calculated and an estimate made of the thickness
of the oil layer, about 10-6 mm. This is an approximate dimension of a single molecule of the
oil.
16. ELECTRICITY
(a) Solids that conduct electricity
The source of the DC supply can be dry cells in series giving 6 volts. The bulb, which should
be low power, indicates when the current is flowing. The electrodes may be carbon or steel,
perhaps mounted in a wooden support, cork or rubber stopper so as to keep the electrodes a
constant distance apart.
(i) Test the conductivity of solids by making a good contact between the surface of the
solid and the two electrodes. The surface of the solid must first be cleaned. All metals
conduct electricity. Carbon conducts electricity. Note whether non-metallic solids, e.g.
plastics, naphthalene, wax, sugar, sodium chloride and sulphur, conduct electricity.
(ii) Glass can be a conductor. Heat a glass rod until it becomes very hot and begins to
soften. Test the hot, soft part with the conductivity apparatus. When molten, glass is a
good conductor of electricity.
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dissolves. Classify substances into the following groups: (a) those which conduct electricity
in the solid state and those which do not; (b) those which conduct in the liquid state and
those which do not; (c) those which conduct when dissolved in water and those which do not
(d) ELECTROLYSIS
In aqueous solutions there are usually four ions present, two from the water and two from
the dissolved salt. The products will be gaseous, or metals which are deposited on the
negative electrode. It is composed of an open cylinder of glass approximately 8 cm high and
2.5 cm in diameter. A small bottle of similar size with the bottom cut off would do just as
well. The cylinder has a 2-hole rubber stopper carrying two carbon electrodes with
connecting leads to a battery, or DC supply of 4 to 6 volts. If cork is used, this must be
made leak proof by covering the whole of the bottom surface round the electrodes and the
glass edge with Faraday's wax or a similar soft wax. The electrodes may be carbon rods
from a dry cell or pencil leads. The alloy supports for the coiled filament in electric light
bulbs have also been found suitable for electrodes. The electrodes should project about 2
cm into the cylinder and also 2 cm below for attaching the leads to the battery. Pencil leads
are brittle, and if they are used it is better to fix the electrodes in the following way.
Solder a piece of stout copper wire to a 4 cm length of braided copper screening wire. Drill
two holes in the rubber stopper with a 1 mm drill. Insert the copper wire into the hole from
above and pull it right through the stopper until the screening wire is also pulled a little way
into the hole. Into the core of this screening wire insert the pencil lead securely. Then pull
the screening wire with the lead further into the stopper so that the lead electrode is
firmly held in the stopper. The excess copper wire is cut off. This procedure is repeated
with the other electrode. The solution is placed in the glass cylinder. The two small tubes
are then filled with the solution, and carefully inverted over the electrodes. The electrodes
are connected to a safe DC supply with a small bulb in series. Increase the voltage until the
bulb lights, showing that a current is flowing. When this happens, cut out the bulb from the
circuit by closing the switch, as shown. This will allow a larger current to flow. The tubes
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collect any gas given off and the properties of the gas should be tested. Using carbon
electrodes, the following results will be found.
Connect the cell to the DC supply and watch for bubbles of gas at both electrodes. If none
appear, add a little more acid or sodium sulphate solution. After 5 to 10 minutes there
should be enough hydrogen and oxygen gas for testing. Predict at which electrode each gas
will appear.
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deposits lead on the cathode and oxygen gas is produced at the anode. If the lead acetate
solution is cloudy, add a few drops of acetic acid. Sodium chloride gives hydrogen gas at the
cathode and chlorine gas at the anode. Copper sulphate deposits copper at the cathode and
oxygen gas is produced at the anode.
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Tin (b) None (c) None
Lead (b) None (c) None
Copper (b) None (c) None
(ii) Recover the zinc after the reaction has ceased. Evaporate the solution to leave zinc
sulphate crystals. Dissolve the colourless zinc sulphate crystals in water and put two carbon
electrodes (central poles of dry cell batteries) in the solution. Connect the electrodes to a
6-volt or 12 volt DC supply. Zinc forms rapidly on the cathode.
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dropper. If the concentration of the acid is known, the concentration of the base can be
estimated by comparing the numbers of drops of acid and drops of base that just react.
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(c) HEAT OF A NEUTRALIZATION REACTION
Dissolve 40 g of sodium hydroxide pellets in water and make up to 500 mL. This is a 2M
solution Also prepare 500 mL of a 2M hydrochloric acid solution. Leave the solutions to cool
to room temperature. Note the actual temperature of the solutions when cool. Then add the
acid to the base quite rapidly and stir with a thermometer. Note the maximum temperature
reached. The increase of temperature should be about 13oC.
(iii) Since the volume of water has been doubled by adding one solution to the other, the
final solution contains 1 mole of OH- (aq) ions which reacted with 1 mole of H+(aq) ions to
form 1 mole of water molecules. We must assume that the specific heat of this moderately
weak solution is the same as that of water.
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(d) the original lumps of marble chips. Place four 100 X 16 mm test tubes in a stand. Weigh
approximately 2 g of each grade, size, of marble chips and put the four grades separately
into each of the four tubes. Obtain four balloons and blow them up several times to stretch
them. Put 5 mL of bench hydrochloric acid into each of the four balloons and slip the mouth
of the balloon over the top of the tube without letting any acid into the tube. When each
balloon is in place, tip the acid into each test-tube at the same time and observe which
balloon is the fastest and the slowest to be blown up. The smallest should give the carbon
dioxide in the shortest time. Instead of using marble chips you can use granulated zinc. Do
not use metals in powder form because the reaction may be too vigorous and even cause an
explosion. Be careful! This reaction produces hydrogen gas! Instead of collecting the gas in
a balloon or plastic bag, a more accurate method would be to collect the gas in a burette
inverted over water and compare the volume of gas given off in unit time for each grade of
marble chips. Another accurate method is to stand a conical flask containing the marble
chips and acid on a balance and record the loss in mass every half minute. Carbon dioxide is
a heavy gas and most balances will enable the loss in mass to be found as the gas escapes.
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solution. Record the final time when the black cross below the beaker is no longer visible.
Repeat the experiment, each time warming the thiosulphate solution to just over 30oC
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water vapour. The ethene is insoluble in water, unlike ethanol, and will collect in the test-
tubes. Test the 3 samples by: (a) burning ethene; (b) shaking with a few drops of dilute
potassium permanganate solution made alkaline with sodium carbonate solution, the colour
should disappear; (c) shaking with a little bromine water, the colour again disappears.
Disconnect the delivery tube when you stop heating to avoid a suck back of water onto the
hot porous pot.
This list given below has been drawn up in order to give guidance to schools concerning the
apparatus that is expected to be generally available per student for examination purposes.
The list is not intended to be exhaustive: in particular, items (such as Bunsen burners,
tripods) that are commonly regarded as standard equipment in a chemical laboratory are not
included in this list.
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Clocks (or wall-clock) to measure to an accuracy of about 1s. (Where clocks are specified,
candidates may use their own wristwatch if they prefer)
Wash bottle
Test tubes (some of which should be Pyrex or hard glass). Approximately
125 mm x 16 mm
Boiling tubes, approximately 150 mm x 25 mm
Stirring rod
ACCURACY
Unless a question instructs candidates differently they should assume that readings from
equipment and apparatus ought to be made with the following precision:
It is important that when candidates record reading they include the appropriate number of
decimal places. For example a burette reading of exactly 24.7 cm3 should be recorded in a
results table as 24.70cm3. A temperature of reading of exactly 350C should be recorded as
35.50C.
When titres have to be averaged, it is important that the mean is expressed to either the
nearest 0.05cm3 or to the second decimal point. For example, if a candidate records four
different titres as listed below, the mean can be worked out.
The candidate is expected to ignore the second titre and average the remaining three
In general, a final should always be given to the same number of significant figures as is
suggested in the exercise.
A significant proportion of marks for quantitative exercise will be awarded for accuracy.
The marks will be awarded by comparing the candidate’s results with the teacher’s reports.
CALCULATIONS
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Usually calculations will be structured. Candidates will be led through a series of steps
leading to a final value. Since most of the marks for these steps will be for a correct
method rather than the numerical answer, it is important that candidates include their
working even if this seems to be trivial. No marks can be awarded for an incorrect answer
without working but a correct method followed by an incorrect answer will receive credit.
GRAPHS
Some exercises in practical chemistry will require candidates to treat their readings
graphically. The question will however instruct the candidate which axes to use for each
quantity being plotted. Some useful points for candidates to keep in mind when constructing
graphs are listed below.
• Candidates will normally be instructed to put the dependent variable, the quantity
being measured e.g. temperature on the y- axis. The predetermined quantity e.g.
volume will be on the x-axis.
• The scales should be chosen so that the results are spread out as far apart as the
size of the grid allows but not at the expense of using a sensible scale. For example
using 1cm to represent 3 units might spread the readings better than using 1 cm to
represent 4 units but the scale may be difficult to read. It is always advisable ton
use even scales.
• The origin (0,0) need not necessarily be included on either scale if it is not relevant.
For example if temperature readings between 210C and 280C are plotted, there is no
need to begin the axes at zero.
• The axes must be clearly labelled with the quantity being plotted e.g. mass and its
units e.g. kilograms
• The points plotted may be joined with a straight line or a smooth curve. Since
readings are all subject to experimental error, the line drawn may not necessarily
pass through every point. Points should never be joined by a series of short straight
lines.
Doing a Titration
Begin by preparing your burette, as described on the burette page. Your burette should be
conditioned and filled with titrant solution. You should check for air bubbles and leaks,
before proceeding with the titration.
Take an initial volume reading and record it in your notebook. Before beginning a titration,
you should always calculate the expected endpoint volume.
Prepare the solution to be analysed by placing it in a clean Erlenmeyer flask or beaker. If
your sample is a solid, make sure it is completely dissolved. Put a magnetic stirrer in the
flask and add indicator. Use the burette to deliver a stream of titrant to within a couple of
mL of your expected endpoint. You will see the indicator change colour when the titrant hits
the solution in the flask, but the colour change disappears upon stirring.
Approach the endpoint more slowly and watch the colour of your flask carefully. Use a wash
bottle to rinse the sides of the flask and the tip of the burette; to be sure all titrant is
mixed in the flask.
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As you approach the endpoint, you may need to add a partial drop of titrant. You can do
this with a rapid spin of a Teflon stopcock or by partially opening the stopcock and rinsing
the partial drop into the flask with a wash bottle. Ask your TA to demonstrate these
techniques for you, in the lab.
Make sure you know what the endpoint should look like. For phenolphthalein, the endpoint is
the first permanent pale pink. The pale pink fades in 10 to 20 minutes.
If you think you might have reached the endpoint, you can record the volume reading and
add another partial drop. Sometimes it is easier to tell when you have gone past the
endpoint.
When you have reached the endpoint, read the final volume in the burette and record it in
your notebook.
Subtract the initial volume to determine the amount of titrant delivered. Use this, the
concentration of the titrant, and the stoichiometry of the titration reaction to calculate
the number of moles of reactant in your analyte solution.
Indicators
An indicator is a substance used in titrations, which has one colour in the presence of an
excess of one reagent and a different colour in the presence of an excess of the other.
Examples of indicators include;
(i) Methyl orange
(ii) Phenolphthalein
(iii) Methyl red
(iv) Bromothymol blue
The pH scale
A much more useful measure of the strength of an acid solution was worked out by the
Danish biochemist S. Sorensen. He worked in the laboratories of the Carlsberg breweries
and was interested in checking the acidity of beer. The scale he introduced was the pH
scale. The scale runs from 1 to 14, and the following general rules apply.
The pH of a solution can be measured in several ways. Universal indicator papers that are
sensitive over the full range of values can be used. Some colour changes of common
indicators are shown below.
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Indicator colour changes
Candidates must follow the health and Safety policy normally operates in their laboratories
when carrying out the practical Examination. Eye protection must always be worn.
Laboratory overalls are recommended. All substances should be regarded as being
potentially toxic and hazardous. Hazard labels (e.g. flammable) should be read and
appropriate precautions (e.g. keep liquid away from flame) taken. All substances spilled on
the skin should be rinsed off immediately. Chemicals must never be tasted Gases and
vapours should never be smelt unless the question instructs the candidates to do so and
then only with great care.
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Amount of substance
In quantitative analysis, it is important to measure the amounts or moles of reacting
substances accurately. To do that, we must use values of relative atomic masses expressed
on a periodic table. If we are given the mass of a compound, we can determine the number
of moles.
The first step is to calculate the mass of one mole of the compound by summing up the
relative atomic masses of the constituent atoms. E.g. 1 mole of calcium carbonate (CaCO3)
will have a mass of 40 + 12 + 48 = 100g
If one mole of a solute is dissolved in water and the volume of the solution made up to 1litre
(1dm3), this solution in known as a molar solution or 1M solution. If two moles are dissolved in
1litre (1dm3), the resulting solution is 2M and so on.
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You need to be able to calculate
(ii) The concentration of an aqueous solution given the amount of substance and
volume of water.
Concentration can also be expressed directly in grams per litre (1dm3). 9.8g of H2SO4 can
be expressed either as 0.1M or 9.8g/dm3
Example 1: 5.95g of potassium bromide were dissolved in 400cm3 of water. Calculate its
molarity. [Ar values: K = 39, Br = 80]
Chemical Equations
These balancing numbers have an additional meaning where these amount calculations are
concerned. The balancing numbers give the numbers of moles present for each chemical
involved in the reaction.
For example, sodium chloride may be prepared by the reaction of sodium hydroxide and
hydrochloric acid, according to the following equation -
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NaOH (aq) + HCl (aq) NaCl (aq) + H2O (l)
The link ed image cannot be display ed. The file may hav e been
mov ed, renamed, or deleted. Verify that the link points to the
correct file and location .
The equation specifies what amounts of sodium hydroxide and hydrochloric acid will react
together and what amounts of products are produced.
This equation states that 1 mol of sodium hydroxide and 1 mol of hydrochloric acid will react
together to give of 1 mol sodium chloride and of 1 mol water.
What this means is that if the amount of any one of the components in the above reaction is
known then the others may be worked out from the ratio above.
Or, if the masses of chemicals reacting together are known then amounts can be calculated
and the balancing numbers deduced from the amounts reacting together.
Titrations can be used to find the concentration of an acid or alkali from the relative
volumes used and the concentration of one of the two reactants.
(i) The acid is poured into the burette. A known volume of the alkali is
transferred using a pipette into four separate conical flasks. Two or three
drops of suitable indicator are added to each of the conical flasks.
(ii) The acid is run into the flask until the indicator just changes colour. The
difference between the initial and final burette readings gives the volume of
the acid used commonly known as the titre. The first titration usually gives
and approximate end point and is treated as the trial.
(iii) The experiment is repeated for each of the other conical flask, to try to
obtain the end point accurately. This is usually done by running out the acid
to a point one unit away from the trial, the going drop-by-drop until an
accurate end point is obtained. The volume of the acid required for each
change is read off and recorded in a table similar to the one below.
Titrations require continuous shaking of the conical flask and its contents.
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Check the quantity of the pipette as indicated on the bulb of the pipette and
remember to record it in the appropriate place.
As you release the liquid from a pipette into a conical flask, one should not blow
out the last drop remaining in the jet.
Before you take any reading from the burette after filling it, first allow the
solution to run out to fill the tap and jet of the burette, and then you begin
taking your readings.
Always write the reading immediately you take them.
When completing the table of results, you will be expected to complete all
columns as accurately as the as the limits of the apparatus can allow e.g.
burette used is usually read to the nearest read to the nearest 0.05 cm 3,
pipette is accurate to 0.05 cm 3 (1 drop).
Use minimum amount of indicator possible (2 – 3 drops) and recognize the end
point has been reached e.g. when the colour just changes.
Show the values that can be averaged to obtain an acceptable value for use in
calculations (only those values within 0.2 cm 3 should be averaged).
Attempt to work out the questions from the first principles and not use the
formula method, which has its own limitations.
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Phenolphthalein Colourless to red 9.5 Strong base-
strong or weak
acid
QUALITATIVE ANALYSIS
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CO2 limewater (aqueous milky white CaCO3(s) +
calcium hydroxide precipitate of H2O(l)
solution) calcium carbonate
Oxygen gas O2 Glowing splint re-ignites it - C(in wood) + O2(g)
flame CO2(g)
Hydrogen chloride (i) Damp blue (i) Litmus turns (i) Litmus turns
gas HCl litmus or red, red,
(ii) Drop of silver
nitrate on the end (ii) White (ii) White
of a glass rod precipitate with precipitate with
silver nitrate silver nitrate
Sulphur dioxide Freshly made Paper changes The dichromate
gas SO2 potassium from orange to (VI) ion, Cr2O72-(aq)
dichromate (VI) green is reduced to the
paper green Cr3+(aq) ion
Ammonia gas NH3 Strong pungent (i) Litmus turns (i) Only common
odour, (i) red blue, (ii) white alkaline gas and (ii)
litmus, (ii) fumes clouds with HCl forms fine
conc. hydrochloric fumes. ammonium chloride
acid crystals with HCl
Chlorine gas Cl2 (i) blue litmus, (ii) pungent green gas, (i) non-metal, is
[test (ii) on its own drop silver nitrate (i) litmus turns red acid in aqueous
is no good, could be on the end of a and then is solution and a
HCl] glass rod bleached white, (ii) powerful oxidising
white precipitate agent, (ii) forms
chloride ion in
water
Nitrogen(IV) oxide No simple Reddish- brown gas Strong oxidising
(or nitrogen relatively agent
dioxide) NO2 unambiguous test
Water vapour H20 (i) White (i) turns from (i) Blue hydrated
anhydrous white to blue, (ii) copper(II) crystals
copper(II) turns from blue to or solution formed,
sulphate, (ii) dry pink (ii) hydrated cobalt
blue cobalt ion formed
chloride paper [Co(H2O)6]2+
Hydrogen sulphide (i)Smell (i)‘Bad eggs’
(ii)Burning splint (ii)Gas burns-
(iii)Lead (II) sulphur deposits
ethanoate paper (iii)Turns brown-
black
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TABLE 2: TEST FOR ANIONS
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(VI) paper sulphites dissolve in acids.
Chloride ion Add dilute White Ag+(aq) + Cl-(aq) AgCl(s).
Cl- nitric acid precipitate of Any soluble silver salt +
and silver silver chloride any soluble chloride
nitrate soluble in dilute silver chloride precipitate.
solution. ammonia.
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salt ammonia should stronger the alkali, the
be released. higher the OH-
concentration, (ii)
ammonia gas is evolved:
NH4+(aq) + OH-(aq) NH3(g)
+ H2O(l)
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colourless solution colourless solution Zn(OH)2(s) white
ppt. The ppt.
dissolves in both
excess sodium
hydroxide and
ammonia to give a
clear colourless
solution.
Lead (Pb2+) White ppt. soluble White ppt.
in excess giving a insoluble in excess
colourless solution
Iron(II) (Fe2+) Green ppt. Green ppt. iron(II) ion: Fe2+(aq)
insoluble in excess insoluble in excess + 2OH-(aq)
Fe(OH)2(s) dark
green ppt. The ppt.
is not soluble in
excess of NH3 or
NaOH.
Iron (III) (Fe3+) Red-brown ppt Red-brown ppt iron(III) ion:
insoluble in excess insoluble in excess Fe3+(aq) + 3OH-(aq)
Fe(OH)3(s) brown
ppt.* The ppt. is
not soluble in
excess of NH3 or
NaOH.
Copper (Cu2+) Light blue ppt. Light blue ppt.
insoluble in excess soluble in excess
giving a deep-blue
solution
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alkanes give no
fast reaction with
bromine)
Hydroxy group R- Mix it with a few Litmus turns red R-OH + CH3COCl
OH in alcohols (in drops of ethanoyl and a white CH3COOR + HCl
'dry' conditions) chloride, test precipitate with An ester and
fumes with litmus silver nitrate, if hydrogen chloride
and silver nitrate the mixture is are formed
poured into water
you may detect a
'pleasant' ester
odour, can test for
HCl but water and
amines produce it
too!
Carboxylic acids Mix with water and Fizzing, colourless RCOOH + NaHCO3
RCOOH add a little sodium gas gives white RCOONa +
hydrogencarbonate precipitate with H2O + CO2
solid or solution limewater
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may also provide precipitate]
clues. The metal
ion solution might zinc carbonate
also give a flame zinc oxide + carbon
colour or a dioxide
hydroxide
precipitate with ZnCO3(s) ZnO(s)
sodium hydroxide + CO2(g)
e.g. copper.
[White] [Yellow
hot, white cold]
+[colourless gas,
test with
limewater, white
precipitate]
Hydrogen ion H+ or (i) litmus or (i) litmus turns (i) PH meter gives
H3O+ universal indicator red, variety of a value of less than
or pH meter, (ii) colours with 7, the lower the
add a little sodium universal indicator. pH number the
hydrogen strong - red, weak stronger the acid,
carbonate powder - yellow/orange, (ii) the higher the H+
fizzing with any concentration, (ii)
carbonate - test HCO3-(aq) + H+(aq)
for CO2 as above H2O(l) + CO2(g)
Ammonium ion no smell at first, Smelly ammonia Ammonia gas is
NH4+ add COLD sodium evolved and red evolved: NH4+(aq) +
hydroxide solution litmus turns blue OH-(aq) NH3(g)
to the suspected + H2O(l)
ammonium salt and
test any gas with
red litmus
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Metal ion Symbol Flame colour
Lithium Li+ Scarlet
Sodium Na+ Yellow
Potassium K+ Lilac
Calcium Ca2+ Brick red
Strontium Sr2+ Crimson
Barium Ba2+ Apple green
Brown gas evolved and a glowing splint Nitrogen dioxide and oxygen from the
relights decomposition of a nitrate
Gas given off which turns limewater cloudy Carbon dioxide from the decomposition
of a carbonate
Pungent gas evolved which turns acid Sulphur dioxide from the decomposition
dichromate paper from orange to green of a sulphate
Sublimate forms on cool part of the tube Likely to be an ammonium salt. (Ammonia
may also be detected with moist red
litmus: it turns it blue.)
Residue turns yellow when hot and then Zinc oxide, which may have been formed
white again when cold by the decomposition of another zinc
compound
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Residue which is red when hot and yellow Led (II) oxide, which may have been
when cold formed by the decomposition of another
lead compound
Soluble Insoluble
Bases The alkalis: sodium and All other metal oxides and hydroxides
potassium hydroxides;
calcium hydroxide, which is
slightly soluble; ammonia.
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TABLE 10 : IGNITION ANALYSIS
Candidates may be asked to heat an unknown alone in an ignition tube. The colour
changes or the identity of any gases evolved may provide evidence as to the
identity of the unknown.
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Hydrogen chloride Hydrated chloride or ammonium chloride
Water Hydrated salts
Soluble Insoluble
Salts
Sodium salts All are soluble None
Potassium salts All are soluble None
Ammonium salts All are soluble None
Chlorides Most are soluble Silver chloride, lead (II)
chloride
Nitrates All are soluble None
Sulphates Most are soluble Barium sulphate, lead (II)
sulphate, calcium sulphate
Ethanoates All are soluble None
Carbonates Sodium, potassium and Most are insoluble
ammonium carbonates
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KEY
Ppt = precipitate
Sol = solution
Insol = insoluble
Xs = excess
Dil = dilute
1.HYDROGEN CHLORIDE
Physical Properties
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Colour Colourless
Chemical Properties
Footnotes:
Dilute hydrochloric acid is one of the three common dilute acids used in the
laboratory.
Concentrated hydrochloric acid is used in the manufacture of many
chemicals.
2.CARBON DIOXIDE
Physical Properties
Colour Colourless
Odour Odourless
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Chemical Properties
Footnotes:
Makes up 0.04% of the gases in the air. Rainwater is slightly acidic because
carbon dioxide dissolves in it.
Needed by green plants during photosynthesis.
Product of respiration in living things.
Product of combustion
Is one of the "greenhouse" gases present in the atmosphere.
Used in fire extinguishers since it is heavier than air and forms a "blanket"
around the fire. This prevents combustion since carbon dioxide does not
support it and the presence of carbon dioxide stops oxygen reaching the
combustible material.
3.CHLORINE GAS
Physical Properties
Colour Greenish-yellow
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Chemical Properties
Footnotes:
One of the "family" of halogen gases (iodine and bromine are in the same
family)
Used in water purification.
Used to make bleaching powder, disinfectants and antiseptics
Also used to make some explosives, poison gases and pesticides.
Physical Properties
Colour Colourless
Chemical Properties
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Solubility in Very soluble in water. It
water reacts with water to form
hydrochloric acid.
Footnotes:
Dilute hydrochloric acid is one of the three common dilute acids used in the
laboratory.
Concentrated hydrochloric acid is used in the manufacture of many
chemicals.
5.HYDROGEN GAS
Physical Properties
Colour Colourless
Odour Odourless
Chemical Properties
Solubility in Insoluble
water
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Red rose petals No reaction
Footnotes:
6.NITROGEN
Physical Properties
Colour Colourless
Odour Odourless
Chemical Properties
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Footnotes:
7.OXYGEN
Physical Properties
Colour Colourless
Odour Odourless
Chemical Properties
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Footnotes:
Physical Properties
Colour Colourless
Chemical Properties
Footnotes:
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